Photoluminescent hybrid materials containing alginate and terbium complex were prepared by a new facile green chemistry method.Terbium complex was covalently grafted to the alginate framework by in-situ synthesis.The preparation was environmentally friendly since it was carried out solely in water at room temperature.Hybrid materials were fabricated as hydrogel,alcogel,xerogel and aerogel.The photoluminescence spectrum of the hybrid materials showed the characteristic green emission of Tb3+ion due to effective “antenna effect”.As shown by SEM,aerogel materials which were obtained by supercritical CO2 drying showed an open network of fibrils 10-15 nm in diameter.